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CAS No. : | 633328-95-7 | MDL No. : | MFCD13193654 |
Formula : | C5H4BrClN2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IIALSLVGUGOODS-UHFFFAOYSA-N |
M.W : | 207.46 | Pubchem ID : | 20600736 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P264-P271-P280-P302+P352-P304+P340+P312-P305+P351+P338-P332+P313-P337+P313-P403+P233-P405-P501 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With triethylamine; In ethanol; at 75.0℃; for 72.0h; | STEP A: (S)-5-Bromo-4-methyl-2-(3-(methylsulfonyl)pyrrolidin-1-yl)pyrimidine [0638] A 40 mL vial was charged with 5-bromo-2-chloro-4-methylpyrimidine (348 mg, 1.675 mmol), (5)-3-(methylsulfonyl)pyrrolidine (250 mg, 1.675 mmol), and Et3N (0.701 mL, 5.03 mmol) in EtOH (90 mL). The resulting yellow solution was stirred at 75C for 3 days. The reaction mixture was partitioned between water (40 mL) and ethyl acetate (40 mL). The organic and aqueous layers were separated, and the aqueous layer was back-extracted with ethyl acetate (75 mL). The organic layers were combined, washed with brine (40 mL), dried over Na2S04, filtered, and concentrated to give the title compound as a white solid, which was used without further purification (430 mg, 80%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With tert.-butylnitrite; N-benzyl-N,N,N-triethylammonium chloride; In dichloromethane; at 25℃; for 2h; | Tert-butyl nitrite (16 g, 155 mmol) was added dropwise to a mixture of <strong>[17321-93-6]5-bromo-4-methyl-2-pyrimidinylamine</strong> (5 g, 26.59 mmol), and benzyltriethylammoniumchloride (27 g, 118.54 mmol) in dichloromethane (200 mL). The reaction mixture was stirred at 25° C. for 2 hours. The reaction mixture was diluted with H2O (50 mL), neutralized with sat. NaHCO3 and extracted with dichloromethane (300 mL×3). All of the dichloromethane layers were combined, dried over Na2SO4, filtered and evaporated. The residue was purified by silica-gel column chromatography (petroleum ether/ethyl acetate=10:1) to give 5-bromo-2-chloro-4-methyl-pyrimidine (2.5 g, 45percent yield) as a white solid. LCMS (ESI) [M+H]+=208.9. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
17% | To a stirred solution of (2-methyl-[l,l*-biphenyl]-3-yl)methanol (7.1 g, 0.036 mol) in DMF (60 mL) at 0C, sodium hydride (1.73 g, 60% in minerali oil, 0.043 mol) was added and stirred at room temperature for 30 minutes. To this mixture, 5- bromo-2-chloro-4-methylpyrimidine (5 g, 0.024 mol) was added and allowed to stir at room temperature for 16h. After completion of the reaction, the reaction mixture was diluted with water (50 mL) and extracted with ethyl acetate (2 x 100 mL). The combined organic layer was then dried over sodium sulfate, filtered and evaporated to give crude product. The crude product was purified on column chromatography (silicagel, 100-200) using 10% ethyl acetate in hexane as eluent to afford 5-bromo-4- methyl-2-((2-methyl-[l, -biphenyl]-3-yl)methoxy)pyrimidine as off-white solid (Yield: 1.5 g, 17%). LCMS (ES) m/z = 369.01 [M+H]+; MR (400 MHz, CDC13): delta 2.31 (s, 3H), 2.58 (s, 3H), 5.47 (s, 2H), 7.21-7.23 (m, 2H), 7.25-7.30 (m, 2H), 7.35 (m, 1H), 7.39-7.43 (m, 2H), 7.49 (m, 1H), 8.47 (s, 1H). HPLC purity 214 nm, 99.78%. |
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